Process of weighting fibers and the product thereof



April 6 1926. 1,579,628

0. BERG ET AL PROCESS OF WEIGHTING FIBERS AND THE PRODUCT THEREOF FiledDec. 26, 1922 A B x C @fm ffil Q fl jQfF/Q fi u zmfin 5n (Z4 Wa/erSod/um Wafer Aluminum W i W fer Wafer Jo/uf/an h P/mp/ml \ju/ v/mfe Glas17 I 1 mm q wyfl o 0 d lead W512 5m Wa/er Acefaiefoiqfibrz Phw /mteJMutian IN VENTOR 02m) fiery Max fmZwjj A TTORNE Y Patented Apr. 6,1926.

UNITED STATES PATENT OFFICE.

' OLAV BERG, OF PATERSON, AND MAXIIIHOFF, OF OLIITON, JERSEY.

Application filed December 28, 1922,. Serial Ro. 609,082. v

To all whom it may concern:

Be it known that we, OLAV BERG, a citizen of Norway, and a resident ofPaterson, Pas saic County, and State of New Jersey, and MAX IMHoFF, acitizen of the United States,

and a resident of Clifton, Passaic County,

and State of New-Jersey, have invented certain new and usefulImprovements in a Process of \Veighting Fibers and the Product Thereof,of which the following is a specification.

This invention relates to the weighting of fibers in general, but moreparticularly to the weighting of silk; weighting being the term of theart for a process of increasing the size and weight of fiber. ,While thepresent process is particularly intended for the treatment of naturalsilk, it is not limited thereto.

Under methods now in vogue and employed in the past, salts of tin, iron,and to a very limited extent, of bismuth and aluminum, have beenrecognized as the only metal salts which could be used in a practicalcommercial way for the Weighting of silk.. Of these, only the salts oftin and iron have been employed'generally; and iron only in the case ofblack or dark colored goods. Heretofore, the extent of weighting hasbeen limited because after a certain amount of weighting material hasbeen taken up, the fiber is injuriously affected. There is a practicallimit in the prior art processes to the amount ofmineral matter whichthe fiber will take up without injuring its physical properties. Usuallythe result was a compromise between increase in quantity and decrease inqualit While by such known processes it has een possible to add tenpercent up to one hundred and thirty percent above pari, above tenpercent the efi'ect on the fibers is markedly 1njurious,'tak ing awayboth elasticity and strength'and mak ing them brittle and tender andsubjectto deterioration with age. While the amount of loadingpermissible in producing commereial Sllk without undue forfeiture ofquality varies with the silk and with, the' operator, twenty-five percent is often considered a practical limlt. 7

The purposes of-the present invention areto improve upon former methodsand to provide an inexpensive and: simple method by which it is possibleto weight silk or other. fibers to any desired extent 'not only withoutmaterially impairing ordestroying, the

essential or desirable qualities thereof, but in fact improving them.Another object is toprovide a new material produced by this process; amaterial which, in the best embodiment of our invention now known to us,is a fiber possessing all the textile qualities of silk but in whichsilk substance may be only a minor fraction; the major being composed oftin and lead oxides and P 0 (phosphoric acid) in some form ofcombination with each other and with the silk substance. The result is asort of composite fiber which, although silky, flexible and strong, andhomogeneous under the microscope, is nevertheless largely mineralmatter.

The lead in the-fiber is fixedly'held and is insoluble. The new fiber,although containing in some embodiments as high as two hundred per centweighting, largely PbO, does not yield lead to boiling vinegar (threeper cent acetic acid) or to any of the liquids I l with which, silk islikely to come in in the dye-house or in use.

One phase of the invention relates to the discovery of a method by whichthere is created in the silk, an aflinity for lead com pounds, making itpossible to combine lead compounds with the fibers in such a way as tomaterially increase its weight and the size of the fiber; that is, so asto give a composite fiber in which a large fraction of the fiber is leadin some form; this composite fibercontact having the desirableproperties of ordinary Weighted silk Without its usual disadvantages andhaving certain new and useful advantages of its own. In this method thesilk or other fibrous material is first treated 1 Fi". '1 indicates thepreliminary weighting;

an preparational-steps and iin which indicates the subsequentweightingsteps.

A special feature of the 'prelimihary or primary wei hting operations,by which the affinity for e heavier nietallic compounds,

is created, is thatthey may be thesame as "heretofore have been employedin tin-weights ing and like processes, so that the apparatus and thematerials now at hand may be eml y ding with'tin may be employed as afirst bath,

namely, a solution of tin tetrachloride (stannic chloride) or of pinksalt, which .is a combination of tin tetrachloride and ammoniumchloride. A solution of sodium stannate has been used in tin weighting.So have potassium or ammonium stannates been used but are not betterthan Sodium stannate. Any of these'materials used in aqueous sois lutiondeposit on the silk a certain amount of tin in a. form equivalent tostannic oxide, SnO Y 3 v i I Tlius in Fig. "1 the fibrous material,which in the'case-of silk may be either in' the gum, .de-gummed' orpartially de-gummed cond1-- tion and may be in the formof fibers, orwoven or knitted fabric, is shown at 5 as passing first into a bath Gota solution of stannic chloride, .(SnCh), then through a wash at 7 ofwater, then into a fixing bath at i 8, such as of sodium phosphate, (NaHPO 12H O),follo wed by another water wash at 9. -In the first bath,which may be, a cold one, as well known, a certain amount of .weight isadded to the fiber andexcess material, stannic chloride and 'HCl, isremoved in the first water wash, (which also maybe cold), the latteralso apparently having to some'extent a hydrolyzing effect on the tinchloride remaining inthe fiber; breaking it up in a way equivalent tothe production oft-iiiv oxide remaining with the fiber and sodiumphosphate is the best substance to times. constitute the first stage ofour complete hydrochloric acid which goes off with the.

water. I a

In place of sodium phosphate other alkalinesalts or carbonates may beused in what we have termed the fixing bath at 8, the

v temperature of this bath being such asthat heretofore used in theart.- In using a phosphate bath, a large amount of P 0 is taken s far asour present knowledge goes,

process and are designated in the drawings as the A stage.

The next stage in "the process may be either that shown atB or thatshown at C in the drawings. The 'stageshown at B is a bath at 10 ofaluminum sulphate vfollowed 'bya'water wash at 11. If this is used. itaddsfiurther weight to the treated material; the accession in weightbeing dueto the taking up of A1 0 The stage designated by the drawingsisa bath ofwatemglass The usual solutions used in weight- 1 at 12 followedby a water wash at 13. This stage also adds to'the weight of the treatedmaterial; SiO being taken up.

The sta B or the stage C follow after the stage has been repeated asmany times as desired. Sometimes both of the stages B and C are utilizedafter the desired treatment by the stage A, but as far as our process isconcerned, the new steps, which we are about to describe as the D stage,may follow directly after the A stage treatment,

after the B stage treatment or after the C stage treatment, (in thelatter case whether or not the B stage treatmenthas been used). Whileour discovery is in the D stage treat.-

for the use of the D stage, and our process therefore comprises somesteps preliminary to the D stage. These preliminary steps may. be, asstated, the old and well known operations used in weighting silk. j

lVe have discovered that the A stage treat ments, preparation of thesilk is required ment, weighting the fibers with tin salts and fixingthem, imparts to the fiber thus treated an affinity. for other metalliccompounds. We have found that the fibers can be further weighted to.practically any desired extent by subjecting themto the treatmentillustrated diagrammatically in Fig. 2. In the best embodiment of ourinvention at present known to' us, the further weighting is donesuitable soluble lead salt, generally lead acetate.

It is possible to use lead salts for this purpose because of the factthat the preparatory treatments described create in the ma terial theproperty of taking up lead (PbO) from them. In the embodiment of our in-.vention herein shown and described, we use at 14 a warm solution oflead acetate, which "may be commercial sugar of lead or a more basicacetate. This, followed by a water wash at 15, is the D stage oftreatment. This D stage increases the weight of the material usuallyfrom 20 per cent to 7 5 'per cent, depending upon the amount of addedmaterials already in the'fiber. The lead acetate furnishes lead whichcombines or unites with the associated fiber and mineral matters andforms an. insoluble compound. The process may terminate here.

\Ve prefer to follow this treatment by the E stage,- -showndiagrammatically, which is subjecting the fibers toa vwarm bath at 16containing sodium phosphate, and then giving the fiber a water wash at17. Sodium phosphate isv the be'st'salt to use at-this stage. Atreatment with sodium phosphate much improves the fiber prepared by thepresent process as so far described.- This E stage not only improves theappearance and the scroop of the fiber. but lmparts to it the propertyof being able to take up more lead compcunds if it is aga n submergedin. the

.with theaid of lead compounds, using any lead acetate solution at 1%.Thus the D stage may be repeated afterthe 'E stage,- again and again, ifdesired. The nency. with which the lead is held in the fiberis increasedby this phosphate aftertreatment. Y By thus alternately adding weightand creating an afiinity or avidity for further weighting material, itis possible to add to the weight of thefiber at an increasing rate to anextent greatly in excess of what has been possible heretofore.

Whether or not the aluminum sulphate or the sodium silicate treatments(B and C) have been employed up to this point, either or both may beused for 'the purpose of a final weighting and fixing treatment. Moreover. these B and C treatments impart to the fiber a further aflinity oravidity for the taking up of more lead salts.

As a concrete example, we have found that with a silk treated with threeapplications of the tin and the phosphate, (the A stage treatment), onehundred pounds of .de-gummed silk fiber which in this stage had addedthirty pounds in'weight, with a single treatment by lead acetate andsodium phosphate (the D and E stages) took on an additional sixty-fivepounds in weight; a second lead acetate treatment (the D stage) addedapproximately fifty pounds in weight and with the aflinity or avidityfor the lead salts further increasedby the sodium phosphate treatment,(the E stage), an additional sixty pounds in weight was added by a thirdtreatment with the lead acetate (the D stage). Another bath in sodiumphosphate after this-put the treated fiber in condition to take upaboutseventy pounds more weight from another bath of lead acetate.

In the present process the weight may be further increased, after'the Dand E stages have been repeated as many times as desired, by giving thetreated fiber another waterglass bath (the C stage). Such a bath alsohas the effect of giving'the material a. still further atfinity for morelead compounds.

The process may be carried on so as to 5 .produce practically anydesired increase in weight with the'important advantage of effectingincreases in weight not only without' injuring the material or causingany substantial deterioration in the mechanical properties or appearanceof the fiber either.

immediately,-in subsequent use or from age, but with some actualmprovement in these respects. 1 The: fibers retain their .flexibilitygand strength. as'well as their appearance and'their ability to take ondyes or be otherwise .treated.. Dyeing is more even. and better and theelasticityis increased. The

. weighted material, furthermoreQhas" good lasting and wearingqualities, the""desiredv scroop, i-s non-poisonous. and is irggplublemAnother important advantage'of the invention is that-this improvedlead-weighting process is applicable to such goods as-are alreadymanufactured so that a manufac turer may makeone .quality of goods, forexample by spinning or weaving, and by giving such goods differentamounts of weight by thisprocess, may make them into any desired numberof different grades by weight. Furthermore, a new and useful materialis'made by this process. p

The drawing and description which we have made of this invention are forillustrative purposes only as we realize that many variations in thesteps and the chemicals employed may be used without departing from thescope of the invention, ,therefore we intend no limitations other thanthose imposed by the appended claims. In the claims we have not includedthe water washing steps as it is understood from this disclosure thatthese follow each bath treatinent.

What we claim is:

' 1. The process of weighting fiber which comprises preliminarilyweighting the fiber any known method which in-' with tin 'b eludes theuse of a fixing bath, and thereafter treating the fiber with a solublelead compound.

2. The process of weighting fiber which comprises preliminarilyweighting the fiber with tin by any known method which includes the useof a fixing bath, then treat-' mg the fiber with a soluble leadcompound,

and thereafter treating the fiber with a fixof a soluble tin compound,treating the same with a soluble phosphate and thereaftertreating thesame with a soluble lead compound.

5.- The process of weighting fiber which I comprises treating the fiberwitha solution of a soluble tin compound and treating the same with afixing bath, to render the treated fiber capable of taking up a lead compound, and thereafter treating thev fiber with asoluble lead compound,then treating the fiber with a soluble phosphate and pound.

6. The process of-weighting'fiber which again-treatingitwith a solublelead" oomcomprisestreating the fiber with a solution of a tin compoundand treating .th'same with a soluble phosphate, to render. -itI capa-..

bleof, taking u'p a lead compound and there after treating it with asoluble lead com pound, then treating it with a soluble phos phate andagain treating it w1th a soluble lead compound. r

7. The process of weighting fiber which comprises treating the fiberwith soluble tin compounds and soluble lead compounds successively withone or more intercalated treatments with solutions of other weightgiving compounds.

8. The process of weighting fiber which comprises mordanting the fiberwith a tin compound and thereafter subjecting lt-to the alternate actionof baths which contain a soluble lead compound and which contain asoluble phosphate.

9. The process of weightingfiber which comprises 'mordanting the fiberwith tin salts, and thereafter subjecting it to repeated successivetreatments with [sodium phosphate and lead acetate baths. p

10. The process of weighting fiber whlch comprises treating the fiberwith a solution of a soluble tin compound and treating the same with'afixing bath, to render the treated fiber capable of taking up a leadcompound, treating the fiber with a soluble lead compound, then treatingthe fiber with a soluble'phosphate and then treating the fiber with awater-glass bath.

11 The process of weighting fiber which comprises forming in the fibercompounds containing tin and containing phosphorus to render the samecapable of taking up a leadcompound, and thereafter treating it witha'soluble lead compound.

12. The process of weighting "comprises forming in the fiber compoundscontaining tin and containing phosphorus to render the same capable oftaking up a lead compound, treating it with a soluble lead compound andthereafter treating it with a fixing bath.

13. The-process of weighting'fiber which comprises'forming in the fibercompounds containing tin and containing phosphorus to render thesame'capable of taking up a lead compound, treating it with a solublelead compound and thereafter treating it" with a soluble phosphate andthen treating it with a water-glass bath.

14:. The process of weighting fiber which comprises forming in the fibercompounds containing tin and containing phosphorus to render the samecapable of taking up a lead compound, and thereafter treating it with asoluble lead compound, then treating it with a soluble phosphate, andagain treating it with a soluble" lead compound,

followed by another phosphate treatment, gndhthereafter treating it w1tha ,water-glass 15. The process of weighting fiber which fiber which witha fixing bath, to'render the treated fiber capable of taking u a leadcompound, treatcompound, thereafter subjecting it to the alternateaction of baths which contain a soluble lead compound and which containa soluble phosphate, and thereafter treating it with a water-glass bath.

17. The process of weighting fiber which comprises treating a fiberwhich contains tin in fixed and insoluble form with a soluble leadcompound.

18. A- textile fiber containing tin an lead y 19. A textile fiber ofwhich at least fifty per cent is tin and lead compounds in fixedcompounds in fixed'and insoluble form;

and insoluble form. 20. A textile'fiber containing compounds of tin,lead and phosphorus;

21. A textile fiber containing tin, lead and phosphorus in fixed andinsoluble" form.

22. A textile'fiber of which at least fifty per cent s tm', leadand-phosphorus in fixed 23. A textile fiber containing substantialamounts of lead in o'xidized. colorless form, said fiber possessing-'fle'xibility,'- resilience and textile strength ;and said lead beingirremo'vablefby the action of warm acetic acid in strength up to liveper cent.- 7

24. A textile fiber containing?substantial amounts of tin and of lead inoxidized color less form, said fiber possessing flexibility, resilienceand textile strength, and said lead being irremovable by the action ofwarm acetic acid in strength up to five per cent.

25. A textile fiber containing substantial amounts of tin and of leadand ofphosphorus in oxidized colorless forms, said fiber possessingtextile properties and said phosphorus and said lead being irremovableby the actionof warm acetic acid in strength up to five per cent.

26. A textile fiber comprising natural silk containing substantialamounts of tin and of lead in oxidized colorless form, said fiberpossessing flexibility, resilience and textile strength, and said leadbeing irremovable by the action of warm acetic acidin strength up tofive per cent.

In witness whereof, I have hereunto set,

December, 1922.

q OLAV BERG. In witness whereof, I have hereunto set my hand this 21"day of December, 1922 MAX IMHoFF.

my hand this 21" day of

